Apparatus for treating an oily liquid with an aqueous liquid



Jan. 31, 1933. E. w. ROTH ET AL APPARATUS FOR TREATING AN OILY LIQUID WITH AN AQUEOUS LIQUID Filed Nov. 4, 1930 3 Sheets-Sheet 1 ww fi WK 8 3 wk w I II .O Q ml HR .8 I I I M I a w h .I SW Wm M I I I I I Q? .I .IIIL. I m I I I T I n I A I W I I I I I m m i I I I a q 5 MI Nu QH N TORS ERNEST W ROTH PAUL W. PRUTZMAN 1% w.

Jan. 31, 1933. ROTH ET AL 1,895,683

APPARATUS FOR TREATING AN OILY LIQUID WITH AN AQUEOUS LIQUID Filed Nov. 4, 1930 3 Sheets-Sheet 2 FIG. 2

ERNEST W- ROTH PAUL W. UTZMAN VENYURS Jan. 31, 1933. ROTH T A 1,895,683

APPARATUS FOR TREATING AN OILY LIQUID WITH AN AQUEOUS LIQUID Filed Nov. 4. 1930 3 Sheets-Sheet 3 FIG. 6

FIG. 7.

' F? F! I A I, J I rao FIG-.8

ERNEST W. ROTH PAUL W. PRUTZMAN ENTORS Patented Jan. 31, 1933 UNiTED STATES PATENT oreica ERNEST W. ROTH AND PAUL W. PRUTZMAN OF LOS ANGELES, CALIFORNIA APPARATUS non TREATING an OILY mourn WITH AN AQUEOUS moon) 7 Application filed November 4, 1930. Serial No. 493,336.-

An object of our invention is to provide means for bringing into chemically reactive contact two mutually immiscible liquids, such as an oil body and an aqueous solution.

An object of our invention is to produce such contact by counter flow, bringing the strongest solution into contact with the most treated oil and fresh 011 into contact with the most exhausted solution.

10 An object of our invention is to produce separate from both the treated and the treating liquid. 7 It is well known that certain tars resulting from the destructive distillation of coal contain phenols and similar bodies which unite,

with sodium hydroXid to form water soluble salts whichmay be broadly classed as phenolates. It is customary to separate the phenols '25' from coal tar distillates by agitating these distillates with an aqueous solution of sodium hydroxid, parting the settled solution from the oil and precipitating the phenols by con tacting with carbon dioxid, by which the sodium is carbonated and the phenols are set free. The object in this case is the recovery of the phenols with the smallest possible con sumption of alkali.

Likewise, when petroleum distillates are All of these bodies unite freely with diluteaqueous alkali (as sodium hydroxid) to form sodium salts, the mixture of reaction products when separated from the 011 being known CO11C6IltIalilOI1: the reaction between the acid treated with strong sulfuric acid and the acid.

colloquially as soap; This product has, very little value and the object of the alkali treatment as applied to petroleum is not the" recovery ofthe soap-but rather the neutralization and purification of the treated oil.

The more limpid and volatile petroleum distillates may as a rule be completely lieu-- tralized and cleansed by agitation with an alkaline solution followed by vigorous wash= ing with water, but the products of cracking operations and the more viscous distillates such as lubricating oils require less energetic treatment to avoid the formation of persistent emulsions. For this there are several r ea-' sons, for example the lubricating-oil soaps, 5', which are freely soluble in water are less soluble in alkaline solutions and may be'separated in a flocculent or'g'elatinous'form if the solution exceeds a certain(but not constant) bodies and the alkali takes place in the oil 1 phase and the reaction product must behydrated and precipitated from the oil before it can dissolve in the aqueous phase-during 7 this hydration and precipitation the soap tends strongly to occlude a material quantity of .oil which, on solution of the soap, sepa rates into microscopic particles which part from the aqueous phase very slowly''and finally, some of 'thereactionproducts are more soluble in oil than in water or aqueous alkali, though as a rule they are also inore soluble in a solution of these soaps than in the oil.

A con sideration of thes e principlesleads to the expectation, which is confirmed by ex perience, that many acid treated' oils will be difiicult or impossible to neutralize and wash by agitation without severe and highly varia ble losses of valuable material-and without the risk of completely emulsifying and losing occasional entire batches. I

7 By the. apparatus and'methods about to be described weareenabled to. completely neutralize acidifiedoils and to completely extract the reaction productstherefrom withouttheloss of any oil and without risk of emulsification. We are also enabled to conduct the neutralizationand washing operations continu- 1 Referring to the ously and with but a trifling amount of regulation or attentlon. v

An apparatus suitable for the practice of my invention is illustrated in the attached drawings, in which Fig. 1 is 'a plan view of the neutralizing and washing pan;

section on the I line section on the line seciion on the section on the,

section on" the line which may well be constructed of galvanized sheet iron, which may be'soldered. r This tray v is. divided into a number of long'andrelative ly narrow troughs Ila-r11 etc, by means of partitions 12 which-reach from top to bottom of the-tray but leave an-opening at alternative ends. Through these troughsthe oil and the alkali solution-(and water)- are flowed in contrary directionsfllie aqueous liquid forming a lowerandthie oil an upper layer.

Theoil' inlet end'of the tray may desirably have a single trough lla'. which is deepe'r-at' one end than the remainder of the trayfThis: is. shown at 13 in Figs. 2, '3 and l. The acid:

oil is admitted to "this-trough through. a pipe lt'and a funnel 15, the top: of the funnel be.-

ingsituated at substantially theupp'er liquid level which is tobe maintained in the tray.

This level may bevaried ifthe funnel is pro vided with a. long thread? 16 running in. a

threaded: sleeve 17 so that the funnel may be screwed upand down. The oil is thusintroduced on-top of the aqueous liquid, which. at this point is 'l-yingquiescent, so that it may 7 "free itself from .any. traces. of suspended oil' without agitation-or disturbance. llhe deepv trough is provided for the purpose of liquid.-

greatly retardingthe flow of theaqueous The upper or oil layer flows in a tortuous course through the various troughs constituting the tray, asindicatedbythe long arrows shown; in Fig. 1.. It finally passes through trough 11k and over the weir 18 (Figs. 1 and 8) into a pocket 19 from which it passes through a pipe 20 to any receptacle for clean oil not shown. The height of this weir fixes theupper liquid level in thetray.

fThe lower or aqueous layer fi'ows'in a contrary tortuous course through the troughs, as

indicated by'th-e short arrows shown in Fig.

1'. In trough 11k (seeFigrl) noaqueous liq uid is introduced as this trough is reserved.

figures, the apparatus consists first of a large shallow box or 'tray10 for the final settlement of traces of water from I the oil. In trough'll water is introduced at the bottom through a pipe 21 controlled by a valve 22. The layer of water thus formed counterfiows the oil to trough 11d (see Fig. 6) where it is withdrawn through a downturned L23, -a nipple 24 and a swing pipe 25, the latter swivelling on an L 26 so that its-end may be raised. or lowered. If this swing pipe be set at the correct height (slightly below the upper surface of the oilin the tray) it will discharge the total flow of .water without draining any oil. I

. An alkaline solution ofthe desired strength is introduced into trough 110 (see Fig. 5') 0 through apipe controlled by a valve 28, I the pipe preferably terminating in a down:

. turned L29. Troughsllc and 11d are separated by means. of a slide 30 retained v the. grooves-31. This slide should extend slightly liquids (the height of which will be the same on each side) but not high enoughto impede the flow of oil over it. l I

The'alkaline solution counterfiows the oil is finally withdrawn from the tray through a pipe 32 and a swing pipe 33v swivelling-on the L 34. 1 Q,

On entering trough-11athe: acid oil, which may contain some pepper acid?- or finely d1- videdacid sludge is brought into-contact with a practically exhausted alkaline sOlution containing salts resulting from pr or neutralization of acid bodies; .911 such contact this pepper acid is preci'pitated'sinks to the-lower part of the trough andlmay'from time to time be withdrawn through pipe 35 andvalve 36. v J. V

Passing in. succession through troughs 11a,

above the upper surface of the two aqueous 1 stream through troughs 11c, 11?) and 11a, and

116 and llothe oil is contacted with progres v sively fresher and stronger alkali (which is'flowing in the opposite direction) and. by the timeit'reachesthe furtherend of trough its acid-content will be completely neutralized. A partofthe resultant soap will be: dissolved in. the alkali, a part will form athin layer between alkali and oil and apart will.

remain dissolved or suspended. in the oil; The

volume relation between these portionswill vary widely withv the nature and acidity of the oil and-is immaterial at this point. Such part of the soap as dissolvesinthe alkali will be carried out of the system through pipe 33 and such parts as form an intermediate layer or remain in the oil are positively carried forward into trough water. y

Suflicient time must be plete neutralization of the acids in this first stage of. the treatment. Contact time'is a factor of depth of oili layer :into flow-rate times length of -passage andimay bacontrolled by feed. Furthe r,contact areamay 11d for treatment with allowed and suiiicient contact must be afforded topermit comlayers.

tralized oil and soap encounters a counterflowing stream of soap solution resulting from prior contact of water with theoil and which, at this point, is escapingfrom trough any soap 'remainlng suspended in'the oil'is hydrolized and caused to settle into the intermediate layer and finally into the water, in which it dissolves withoutcarrying'any oil with it. Flowing alongtroughs 11d,"116 and so on through trough llj theoil layer is contacted with progressively purer -water, the soap being thus gradually eliminated and passed into the counterfiowing water stream.

The oil finally passes into the end trough 1170 where it is afi'orded an opportunity to settle completely and finally passes overweir 18 into the finished oil outlet 20. 7

It will be understood that the number and the relative proportions of the troughsshown in the figure are purely illustrative and that the apparatus will be, in practiceppropor tioned to the kind of oil to be treated andto the capacity required. In particular, the depth of the respective layers is considerably exaggerated in the drawings, the rate of flow of such thick layers being too slow'to afford the most effectivecontact between the two If in any given apparatus .theextent of contact is not sufiicient to produce a complete,

neutralization or a satisfactory washing of the oil at the desired rate of flow, several means 'for increasing contact are available. These are all designed to break and disturb the plane of contact between oil and aqueous liquid. This plane is liable to accumulate the mentioned intermediate layer of precipitated soap which, in its hydrolized condition, is often of a gelatinous consistency and not readily brought into solution. I

Thus in trough 112' we show a pipe lying along the bottom and having upward looking perforations, which should be of very small diameter. If such a pipe be located near the oil outlet end of the apparatus, where the oil has already been largely deprived of soap, this pipe may be supplied withvair under pressure and the water thus thoroughly agitated with the oil before the latter passes to the settling trough 1170. This treatment would be too strenuous for oil containing considerable soap, as it might lead to emulsification, and a moderated action may be produced in such case by supplying the pipe with water under a low pressure, the needlejets ot-v water thus e ected causing the water layer to I above described 1 disturbingor acceleratingwell up'and gently wash the oil.

A highly desirable breaking up and dissemination of the intermediate soap layer may be produced by the bafiles shown in Figs.

1 and 3 in troughsill euand 11f. Inthe former the soap layer is caused to string through narrow vertical slots in battles 37 which are placed across the-contact line, the viscosity ofthe soap causing it to be retarded and banked up by the bafile and thelower portion of the strip l passing through the slot Pbeing thus forced beneath the surface of thejwater. A 11d throughpipe 25. Bythis initial contact strip of wire screen of say mesh may be used with substantiallythe same result,-

. In the latter'a plain .bafi'l'e- 38 is used which forces thesoap layer to pass, at least in part,

under its loweredge,this effect being accentu atedf if: the 'bafile'fiis sloped so that its lower edge 18 downstream tothe waterflow. These; baffles, whichneed be no more than StllPS'Of so I J light sheet i11etal-,"1 nay be slid-into slots formed. by opposing two: verylight angle f vdicatedat llinFig.

The eiiiciency of contact may also be inboth of the-liquids. In trough lle (Figs. 1

the-passage of only the oil, causing it to take circuitous course through each individual 9Q e creased by increasing tlievelo city of one or and a wing bathe is shown which obstructs i trough while the aqueous liquid flows beneath it in a straight line. 1ntr-ough llfthe baffle 1s' shlown as obstructing the course -ot the aqueous liquid and, ifthe b'ai e beof'the same:

depth {asithe trough, the maximum effect of increasing the vel citycfboth liquids is'ob-j jtamed; By proper spa'clng and immersion of'sucli-bafiies, according tothe nature ofthe materials, eddy currentsmay' be set up by which hlghly 'QflGClZlVB contact maybe obtained without jdanger-oiiproducing an mulsio'n orapersistent su'spension of either liquid'in the "other. V s v I desirable'towithdraw I 27, asthe addition of alkali will often throwv "In most cases it 1s the wash water at '24 before adding alkali at the dissolvedseap outot solution; In such' casethe slide 30 is closed'as indicated in. Fig.

5; In some cases, however, the wash water reaching outlet 24 will carry material quantities of oil,'due to excessive agitation or disturbance in the Water washing troughs;

In such case theslidemay bewithdrawn and v I swing-pipe 25'sufiic1ently raised to prevent the outflow ofwaterQ The soap solution will thus be 'detoured into contact withthe Center v oil will be rejected andicausedto rise'intothe ing alkali solution, by which the entrained,

supernatant oil layer,whilethesoapwill pass to the outlet 33 along with t 1e alkali. It wi'll be understood that anyor all ofthe' I means may be appliedl'inanyior. all (if-the troughs as they may be requiredin specific c'asesand thatthe most flexible andgenerally a '40 7 4.- Apparatus substantlally asand'for the' 5o 7 for Withdraingan aqueousliquid and-subuseful apparatus wivillbe supplied withjbalile J with an aqueous liquid, comprising; a series, 1 across, a trough and extendingiabove and v '10 v liquid entering one"end i ofsaidsseries,and a slotsi'and with air a an d, Waterco'nnections in each trough for "use in such combination as may "be' -found to give the best results in each in i i I c. .VVe'claim as our invention: 1 a 1. Apparatus for treating an oily liquid of'adjoining troughs communicating'at alter-4 nate ends; a pipe for introducing an aqueous pipe for witndrawing said-liquid connected to.

" said aqueousl'iquid atfir'st'saidend; of said .the opposite end of said series; meansjfor in- 'troducing an ioily liquid over "said aqueous 15 liquid a't'last said end of sa-i'dseries andm'eans for w thdrawing Said ollyf llquld from ofver series, whereby said oilyfliquid is' causedto counte1flow over the surface ofsaid aqueous 2 liquid; throughout said series. I

2.".Apparatus for treating an] oily liquid With an aqueous liquid, c-omprising a series (if-adjoining troughsv comnumicating at al; ternate ends; means including inlet-and exit pipes each directly communicating with one of. said troughs for flowing a layerof aqueous liquid over the bottomof said/series in one directionand means including inlet and exit "pipes, each directly communicating Withone 30 liquid over saidjacuieouslayer inanopposite of said'troughs for flowing a layer of oily direction,whereby said liquids are ,continjuou'sl-y contacted at the substantiallylhorizon 'tal interfaceofsaidlayers; 1 i; ,-:3. Apparatussubstantially as and forthe V purpose set forth infclaim 2, including funnel into said pipej q r. Witness that wecla-im the foregoing we, 7 have hereunto subscribed our naines this 28th liquids.

9. Apparatus:substantially gas and for 1 v i purpose set forth in claim 2, including vlea-file plates affixed to' alternate sides of a trough 9 for'ink zreasing.the rate of flow of'said liquids.

' 10. Apparatus substantially as" and for/the purpose set forth in cla'im2, including bafiies below the interface between Esaidlayers.

11; [Apparatus substantially as and for the lower edges ofzsaid bafllesbeing serrated.

a 12. Apparatussubstantially as and-fori'the v v purpose set'forth-in claim 2, including perfo-j rate .bafiles across atrough and extending above and below the interface between said layers. a r

" 13. Appar "tus substantially as andforthe purpose set forth in claim 2, including a per' foratepipe laidxlongitudinally in the bottom r of atroug andmeans for intro'ducing'a fluid day of; Oct.,;1930. H ERNEST W ROTH; J

" j PRUTZMAN.

means for introducing; a flow of oil into said i oily layer, WlthOIlt disturbing said aqueous layer;said funnel being arranged for upward fiow ofoil therethrough.

purpose set forth in claim 2, including a i V trough materially deepened at the {end at 5'. Apparatus susbtantially as and'for the purpose, set forth in claim 2,'including meanslocated intermediate the ends of said, series stit'uting' another aqueous liquid therefor. 6. Apparatus substantially as and for the purpose set. forth in claim 2, inc'ludin'g means 7 located intermediate the-ends ofsaid seriesfor introducing a second aqueous-liquid'into a up: a

- the flowing layer .offirst saicl'aqueous liquid? V E es '7. Apparatus substantiallyas and for the a purposeiset forthin claim 2, including means.

for disturbing the interface -';between "said layers for increasing. the areal'of contact'bee;

tween said layers; i-

8."Apparatus substantially as andvfor'the purpose-set forth inclaim 2, including bafiie' plates aifixed to"alternatesides'of a tlfougli I if u 

